PREPARATION OF KETENE FROM GLACIAL ACETIC ACID. METHYL ACETATE, AND ETHYL ACETATE
PREPARATION OF KETENE FROM GLACIAL ACETIC ACID. METHYL ACETATE, AND ETHYL ACETATE
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由冰醋酸制备乙烯酮。
DOI：
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发表时间：
1952
期刊：
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通讯作者：
K. K. Georgieff
中科院分区：
文献类型：
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作者：
K. K. Georgieff
进行了实验室研究，以确定乙酸甲酯和乙酸乙酯是否可以热解，得到的收率和转化率为乙烯酮可比的那些从乙酸。在0.33%磷酸三乙酯或磷酸催化剂存在下，在680°-760 °C下，乙酸热解成乙烯酮和水。140-160 mm。 绝对汞。最高收率为80.6%，最高转化率为34.5%。乙酸甲酯在610°-685 °C裂解成乙烯酮和甲醇。95-400毫米。 无水，使用磷酸三乙酯、磷酸、硫酸、硫酸二甲酯、硼酸丁酯和硅胶硼酸作为催化剂。只有在2-3%的磷酸盐浓度下才能获得高产率。乙烯酮的最大产率（包括作为乙酸回收的乙烯酮）为76%（转化率31-34%）。甲醇的最大产率为81.3%（转化率为33-34%）。含有18%甲醇的乙酸甲酯也被裂化，但结果较差。在0.33%磷酸三乙酯存在下，乙酸乙酯热分解为乙酸乙酯。
Laboratory studies were carried out to determine whether methyl and ethyl acetates could be pyrolyzed to give yields and conversions to ketene comparable to those obtainable from acetic acid. Acetic acid was pyrolyzed to ketene and water in the presence of 0.33% triethyl phosphate or phosphoric acid catalyst at 680°–760 °C. and 140–160 mm. Hg absolute. Maximum yield obtained was 80.6% and maximum conversion 34.5%. Methyl acetate was cracked to ketene and methanol at 610°–685 °C. and 95–400 mm. absolute, using triethyl phosphate, phosphoric acid, sulphuric acid, dimethyl sulphate, butyl borate, and silica gelboric acid as catalysts. High yields could be obtained only with phosphates in 2–3% concentration. Maximum yield to ketene, including ketene recovered as acetic acid, was 76% (conversion 31–34%). Maximum yield to methanol was 81.3% (conversion 33–34%). Methyl acetate containing 18% methanol was also cracked but results were poorer. Ethyl acetate, in the presence of 0.33% triethyl phosphate, was pyrolyz...